反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3,5-Di-t-butylbromobenzene (10 g, 37 mmol) and magnesium (1.8 g, 75 mmol) were dissolved in 100 mL of THF and stirred at reflux for five hours. After this time, triisopropylborate (7.0 g, 37 mmol) as a solution in diethylether (50 mL) was added to the solution, followed by stirring at room temperature overnight. Then the THF was removed in vacuo to leave a crude oil. This oil was taken up in 100 mL of diethylether and 100 mL of 10% sulfuric acid (aqueous) and stirred for two hours. The organic layer was separated and neutralized with saturated sodium bicarbonate solution, whereafter the solvent was removed in vacuo to yield a white solid. The solid is washed generously with pentane. Yield: 3.0 g (34%).
WORKUP
后处理
- temperatureat reflux for five hours
- stirringby stirring at room temperature overnight
- customThen the THF was removed in vacuo
- customto leave a crude oil
- customThe organic layer was separated
- customwas removed in vacuo
- customto yield a white solid
- washThe solid is washed generously with pentane